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By M. M. Wong

Salt mixtures consisting of KC1, BaC12, and HfCl4 with RbCl or CsCl were investigated as electrolytes for refining hafnium. The presence of RbCI or CsCl in the electrolyte appeared to suppress the volatility of. Best electrorefining was obtained with an electrolyte containing 50.7 percent KCl, 27.l percent BaCl2, 15.7 percent CsCl, and 6.5 percent HfCl4. In this electrolyte, hafnium metal with an average oxygen content of 470 ppm was produced from an anode feed containing l,600 ppm oxygen. All metallic impurities were lowered, except titanium, manganese, and tin.

Jan 1, 1966

By C. M. McKinney

The Bureau of Mines analyzed 626 crude oils from 546 oilfields in the United States that produced 2,500 BOPD or more during at least 1 of the last 3 years. Included also are crude oil analyses from eight fields that produced less but which were located in areas having few or no fields that produced 2,500 BOPD. The tables show the geographical and geological source, general characteristics. and determined and computed analytical data for each sample. The analyses were made according to the Bureau of Mines routine method and are directly comparable to other previously published analyses.

Jan 1, 1966

By Kenneth R. Farley

The Bureau of Mines developed a rapid and accurate flame photometric procedure for determining cesium and rubidium in ores and in products associated with the extractive metallurgy of these elements. The effect of associated ions is neutralized by addition of buffer solution; alkali metal effects are neutralized by parallel analyses made on standard solutions similar in composition to the sample being studied. The overall accuracy of the method is within 2.5 pct of the amount of cesium or rubidium present; the range from 1 to 25 pct is the most accurate.

Jan 1, 1966

By J. A. Cavallaro

To determine whether magnetite consumption could be reduced and salable coal production increased by using froth flotation units in series with magnetic separators, the Bureau of Mines conducted laboratory froth flotation tests on primary magnetic separator effluents obtained from three coal preparation plants. Tests were performed in a standard 500-gram-capacity laboratory batch flotation cell. Oleic acid and methylisobutyl carbinol were used as the collector and frother, respectively. Magnetite recovery was comparable to that expected from secondary magnetic separation, and salable float coal recoveries of 0,8 to 7.6 tons per hour were obtainable. The economics of the proposed technique appear to be sound.

Jan 1, 1966

By J. A. Cavallaro

The heats of formation of anhydrous barium carbonate (witherite), strontium carbonate (strontianite), and lead carbonate (cerussite) were determined by solution calorimetry. The solution mediums were hydrochloric acid for barium and strontium carbonates and perchloric acid for lead carbonate. The heats of formation at 298.15° K are as follows: BaCO3 -297.5 ± 0.8 kcal/mole; SrCO3 -294.6 ± 0.5 kcal/mole; and PbCO3 -168.0 ± 0.3 kcal/mole.

Jan 1, 1966

By T. S. Chen

A study was made by the Bureau of Mines of the temperature and thermal stress distributions in thin circular disks subjected to peripheral thermal shock at various rates of heat transfer. The theoretical analysis is based on one-dimensional radial heat flow by conduction in the disk, and on heat exchange by convection between the disk and its surroundings. Preliminary experimental data obtained from shock tests on thin circular disks of basalt, quartzite, and taconite show reasonably good agreement with theory. The case of constant properties and plane stress is treated. Solutions of the stress distribution are presented for both cooling and heating shocks. The elastic energy stored at fracture is examined, and on this basis an average stress theory is formulated. Physical properties vital to the studies include thermal conductivity, thermal diffusivity, tensile strength, Young's modulus, and linear coefficient of thermal expansion. This work is of importance in predicting the thermal shock responses of a rock body of finite size.

Jan 1, 1966

By Earle S. Burnett

Rotating piston deadweight gages have been used for many years for measurement of pressure to several hundred atmospheres. They have been calibrated by comparison of fluid pressures produced by various loads bearing on the piston bases, as measured by corresponding heights of balancing columns of mercury. When expressed in appropriate units, these ratios of column heights to piston loads are called piston constants. Experimental arrangements and procedures for their determination are presented in this paper, followed by a discussion of their significance and of their subsequent applications.

Jan 1, 1966

By A. W. Deurbrouck

This report describes the preparation characteristics of the significant coalbeds from which samples could be obtained in Webster County, W. Va. In 1964, approximately 825,000 tons of coal was produced in the county, of which 732,000 tons was mechanically cleaned in three preparation plants. The Sewell coal bed accounted for 94 percent of the coal produced. Twelve samples were collected from five coalbeds. Four of the samples would require upgrading to meet metallurgical requirements; two others of just over 8.0 percent ash would require some upgrading. In general the coalbed samples collected in the county were of medium-sulfur and medium-to low-ash content as received or after removal of the sink 1.58-specific-gravity material.

Jan 1, 1966

By Erie C. Donaldson

Gas-displacement tests were made in Berea Sandstone and Arbuckle Lime-stone cores to determine the relative permeabilities to gas, oil, and water for two-and three-phase dynamic systems. Three-phase relative permeabilities were obtained by displacing oil and water from the core with gas and measuring the flow rates of the three fluids simultaneously. It was found that relative permeabilities to fluids in a porous medium are affected by the saturation distributions of other fluids in the medium as well as by their own saturation distributions.

Jan 1, 1966

By J. P. Hansen

Reducibility tests were run by the Bureau of Mines on an open hearth lump ore and four groups of pellets whose smelting characteristics had been deter-mined previously in the Bureau's experimental blast furnace. When reduction data from various tests were plotted on specially prepared paper l-(l-percent reduction/100)1/3 against time, the plots were linear. The iron-wustite inter-face therefore advances at a constant rate. The rate of the interface advance in mm/min was used as a reducibility index. The reducibility index measured at 900° C, using 0.45 cu ft hydrogen per minute varied inversely with the surface area of the sample. Even with carefully controlled surface areas, how-ever, duplicate reducibility indices varied considerably. When enough tests were run to give a stable mean, the mean reducibility index did correlate with blast furnace production for the four pellet groups. Results indicated that if the interface speed itself were to be used for correlation with blast furnace production, a sample size of about 180 grams of minus 0.742-plus 0.525-inch particles should be used with a test temperature of 900° C and a flow of 0.45 cu ft hydrogen per minute.

Jan 1, 1966

By Henry C. Meeves

The nonpegmatitic sources of beryllium in Arizona, Colorado, New Mexico, Utah, and four adjacent states investigated by the Bureau of Mines are described. The investigations included 155 properties from which over 6,200 rock samples were collected; more than 5,500 samples were analyzed by the nuclear beryllium-detection technique. Twenty-four of the properties examined had rock containing more than 0.10 percent BeO. Many of the beryllium determinations were made in the field with portable detection instruments by direct scanning of outcrops and by testing samples of rock brought to the instrument. The large domestic resources of low-grade nonpegmatitic beryllium ore in Utah, which were discovered by private enterprise and which respond favorably to small-scale treatment processes, may come into commercial use and thus reduce the dependence of the United States on imported beryl.

Jan 1, 1966

By Walter Kawa

Coals of various rank were reacted by the Bureau of Nines in plasma jets generated from argon and argon-hydrogen mixtures containing up to 33 volume-percent hydrogen. Average plasma temperatures ranged from about 3,400° to 12,000° C. Products were a solid residue and a gas containing hydrogen, methane, acetylene, diacetylene, and oxides of carbon. The highest yield of acetylene obtained with argon plasmas was 15 percent by weight of moisture- and ash-free coal. The data indicated that acetylene yields of 40 percent or higher can be obtained from the reaction of coal in argon-hydrogen plasmas, although results from these experiments could not be correlated with operating variables because of low recoveries plasma contained sufficient energy to heat the coal to temperatures as high 9,000 or 10,000° C, but complete devolatilization did not occur in any experiment.

Jan 1, 1966

By Donald R. Corson

The Bureau of Mines is conducting research on the effects of various established and potential soil-stabilization additives to hydraulic backfill. This initial phase is an evaluation of the effect of inclusion of varying amounts of Portland cement and combinations of cement and a dispersant on the bearing strength of backfill. Results of unconfined compression tests are given for over 200 sample cylinders incorporating a fill material with cement or cement and dispersant. Inclusion of a minor amount of dispersant (0.2 percent by weight) is found to yield a significant increase in strength for 20-to-1 and leaner sand-cement mixes. An apparent optimum concentration of dispersant exists beyond which no further increase in strength is achieved. A dispersant-cement ratio of l.8- to-1 yielded a strength increase of 515 percent over the strength of untreated 40-to-l sand-cement mixes.

Jan 1, 1966

By S. E. Khalafallo

The Bureau of Mines investigated the kinetics of reduction of wustite and magnetite with carbon monoxide. A mechanism was postulated wherein the interaction between gaseous and absorbed carbon monoxide appears to be the rate-determining process. This mechanism fully accounts for the experimental rate equation JL.h relates th velocity of reduction to the pressure of the reducing gas at constant temperature. It also explains the variability of the heat of activation of the reduction process with the state of aggregation of the oxide material. The integrated rate equation is in perfect agreement with the experimental reduction-time curves.

Jan 1, 1966

By Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

Jan 1, 1966

By H. J. Heinen

The Bureau of Milts studied repetitive batch electrowinning of molybdenum from molybdic oxide ) to determine the effects upon the electrolyte life, purity of metal product , and overall cell performance. The electrolyte consisted of 54.0 weight-percent sodium tetraborate (Na2B407), 23.6 weight-percent sodium chloride (NaC1), 14.9 weight-percent sodium fluoride (NaF), and 7.5 weight-percent Mo03. The feed materials were pure and technical-grade Mo03. Electrolysis was conducted at l,000° C in a graphite cell in an atmosphere of air and carbon oxides. Electrolyte degradation did not occur during repetitive winning of molybdenum from pure Mo03 in an 8-day (5,400-ampere-hour) period of operation. Electrowon metal contained <0.1 percent total impurities. The electrode configuration is a key factor in the direct conversion of technical-grade Mo03 to metal by repetitive cyclic electrolysis. The best configuration found was a cathodic crucible and a central anode. Metal purity of 99.8 percent and a current efficiency of 91 percent were maintained until the combined impurity buildup the electrolyte reached 4.7 percent silicon, l.0 percent aluminum, and 0.6 percent iron. One pound of molybdenum was produced per 1.5 pounds of solvent salts employed. About 25 percent of the initial NaCl and NaF contents of the electrolyte were lost owing to volatilization and crucible penetration.

Jan 1, 1966

By J. E. Tress

The Bureau of Mines prepared submicron tungsten powder by reducing tungsten hexachloride with hydrogen. The particle diameters of the resulting tungsten powders ranged from 0.015 to 0.046 micron. Within the limits of the variables investigated, no clear-cut correlation was found between process conditions and final size of the powder. Oxygen was the major contaminant in the product; being present both as an adsorbed gas and as suboxides of tungsten. Studies showed that the powder yielded compacts of approximately 45 per-cent of theoretical density when compacted mechanically. Low-temperature sintering produced more rapid densification in these compacts than in compacts prepared from conventional powders. Adding up to 20 percent ultrafine powder to conventional tungsten powder caused an increase in density upon compaction with maximum densification occurring at approximately 12 percent ultrafine powder.

Jan 1, 1966

By Bernard Porter

The densities of LiF, NaF, and KF, of binary mixtures of these alkali fluorides, and of binary mixtures of UF4, ThF4, YF3, LaF3, and CeF with each of tie alkali fluorides were measured as functions of the melt composition and temperature. Molar volumes at 1,000° C were calculated for all the mixtures. Binary systems containing LiF exhibited molar volume ideality. Binary fluoride systems containing either NaF or KF as the alkali fluoride exhibit positive deviations from molar volume additivity. However, molar volumes in the NaF-KF system are ideal.

Jan 1, 1966

By Donald W. Mitchell

Certification tests for urethane-foam systems and techniques for apply-ing foam safely in mines are described. Fire hazard from foam exists if flame propagates beyond the ignition source or penetrates the foam. Foam that passes the certification tests can be applied on stoppings, continuous sections of ribs of relatively wide passageways (with no foam on the roof), short sections of roof such as overcasts, roof cavities, and intersections (with no foam on the ribs), and between buntons on one wall of a shaft. Foam on the ribs and adjoining roof presents a fire hazard. Stoppings covered with foam passing the certification tests are resistant to penetration of heat, flame, and smoke than similar stopping without foam. Flame propagation can be arrested by water sprays. Spontaneous ignition of foam can be prevented.

Jan 1, 1966

By James Paone

The Bureau of Mines studied the behavior of rocks at the initial state of crater formation that results from the stresses created under a drill bit to determine which mechanical properties of rock are important in rock fragmentation by drilling. Although a definite relation between the drilling strength and relevant mechanical properties has not been established, maximum yield strength of rock is apparently a parameter of drillability of rock. The strengths of rock were considered from the Mohr-Coulomb criterion from which the surface of failure was constructed. The results from previous tri-axial tests on Solenhofen limestone were adopted to verify the criterion of failure. Inelastic behavior of some rock types was observed under a low-velocity impact of a hemispherical bit and under static indentation with a similar bit. Quantitative determinations of strengths of Solenhofen limestone) Indiana limestone, and Tennessee marble were made under static indentation. The maximum yield strength estimated from the average stress over the indented area was used as the crushing strength of rock under a drill bit.

Jan 1, 1966